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United States Patent |
6,071,349
|
Kurosawa
,   et al.
|
June 6, 2000
|
Gas supplying apparatus and vapor-phase growth plant
Abstract
A vapor-phase growth plant which has a dopant gas supplying apparatus
comprising a plurality of dopant gas supplying containers, and a multiple
stage gas flow subsystem with a plurality of dopant gas supply conduits
therein, of which said dopant gas supply conduits form a tournament-style
network with a plurality of confluences on which the dopant gas supply
conduits are united and the gas flows therein are merged for subjection to
even mixing which results in gradual decreasing of the number of the
dopant gas supply conduits as the dopant gas flows proceed in the multiple
stage gas flow subsystem. Together with the equipped pressure reducing
valves, the dopant gas which is highly evened in its pressure and its
concentration can be supplied to the vapor-phase growth apparatus, thereby
affording stable production of vapor-phase growth products with extremely
lessened quality variance. The dopant gas supplying apparatus described
compiles the gas supply conduits within it to two groups, each of which
can be used alternatively by switching of these. Therefore, the apparatus
can supply dopant gas continuously and for a longer period. Also the
operation of the dopant gas supplying apparatus can be simplified.
Inventors:
|
Kurosawa; Yasushi (Annaka, JP);
Oguro; Kyoji (Nishishirakawa-gun, JP);
Ota; Yutaka (Annaka, JP);
Okubo; Yuji (Annaka, JP)
|
Assignee:
|
Shin-Etsu Handotai Co., Ltd. (Tokyo, JP)
|
Appl. No.:
|
893540 |
Filed:
|
July 11, 1997 |
Foreign Application Priority Data
Current U.S. Class: |
118/715; 156/345.29 |
Intern'l Class: |
C23C 016/00 |
Field of Search: |
118/715
156/345
|
References Cited
U.S. Patent Documents
5244500 | Sep., 1993 | Ebata | 118/697.
|
5470390 | Nov., 1995 | Nishikawa et al. | 118/719.
|
5517943 | May., 1996 | Takahashi | 118/715.
|
Primary Examiner: Bueker; Richard
Assistant Examiner: Fieler; Erin
Attorney, Agent or Firm: Snider & Associates, Snider; Ronald R.
Claims
What is claimed is:
1. A gas supplying apparatus for supplying high pressure dopant gas flowing
from gas supplying containers which are filled with a single dopant gas
therein, through gas conduction means equipped with pressure reducing
valves, to at least one chemical processing apparatus, the gas supplying
apparatus comprising:
(a) a plurality of single dopant gas type supplying containers each of
which having an outlet for simultaneous supplying of said single dopant
gas flow therefrom; and
(b) a gas conduction means for conducting said single dopant gas flow
having a plurality of gas supply conduits each of which being connected to
each outlet of said gas supplying containers, wherein the gas supply
conduits form a multiple stage network with a plurality of confluences
which merge and unite said gas supply conduits respectively along with a
gas flow direction, thereby reducing the number of gas supply conduits,
wherein a final stage of said multiple stage network is formed at a final
stage confluence of single gas type supply conduits thereof,
wherein the final stage confluence is connected through at least one
pressure reducing valve to at least one chemical processing apparatus,
wherein dopant gas flow rate of each single dopant gas supplying container
flows evenly out therefrom, and
wherein there is an even pressure drop within said gas supply conduits
jointly connected between each of said outlets of each said gas supplying
containers and said final stage confluence therethrough.
2. A gas supplying apparatus as in claim 1 wherein the gas conduction means
gas supply conduits comprise a multiple stage tournament style network,
formed by merging and uniting said gas supply conduits on said respective
confluences.
3. A gas supplying apparatus as in claim 1, further comprising at least one
gas buffering means inserted between an outlet of said pressure reducing
valve at the final stage confluence and respective chemical processing
apparatus.
4. A gas supplying apparatus as in claim 1, further comprising at least one
gas purging apparatus equipped with at least one purging gas supplying
conduit with at least one purging gas discharge conduit and with at least
one decompression exhaust conduit.
5. A gas supplying apparatus as in claim 1, in which said each gas
supplying conduit has the same inner diameter and the same length and the
same bending configuration so as to provide an even pressure drop within
said gas conduction means disposed between said each gas supplying
container and respective said confluence.
6. A gas supplying apparatus as in claim 1, wherein said chemical
processing apparatus is a vapor-phase growth apparatus.
7. A vapor-phase growth plant having at least one gas supplying container
containing a high pressure dopant gas, at least one vapor-phrase growth
apparatus and a dopant gas conduction means together with at least one
pressure reducing valve, for growing a thin film in the presence of said
dopant gas supplied by said dopant gas conduction means on substrate
disposed within said vapor-phase growth apparatus, the vapor growth plant
comprising:
(a) a plurality of single dopant gas supplying containers each having an
outlet for simultaneously supplying said single dopant gas flow; and
(b) a gas conduction means for conducting said single dopant gas flow
having a plurality of gas supply conduits each of which is connected to
each outlet of said single dopant gas supplying containers,
wherein the gas supply conduits form a multiple stage network with a
plurality of confluences which merge and unite said gas supply conduits
along with said single dopant gas flow, thereby reducing the number of gas
supply conduits, wherein the final stage of said multiple stage network is
formed at the final stage confluence of single dopant gas supply conduit,
wherein the final confluence is connected through at least one pressure
reducing valve to at least one vapor-phase growth apparatus,
wherein single dopant gas flow rate of said each gas supplying container
flows evenly out therefrom, and
wherein there is an even pressure drop within said single dopant gas supply
conduits jointly connected between each of said outlet of each said single
dopant gas supplying containers and said final stage confluence.
8. A vapor growth plant as in claim 7 wherein the thin film is a single
crystalline silicon semiconductor thin film.
Description
The present disclosure relates to subject matter contained in Japanese
patent application No. 202959/1996/ (filed on Jul. 12, 1996) which is
expressly incorporated herein by reference in its entirety.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a gas supplying apparatus for supplying high
pressure gas flowing from gas containers to chemical processing apparatus
by reducing said gas pressure.
Moreover, this invention relates to a vapor-phase growth plant comprising a
dopant gas conduction means for supplying high pressure dopant gas flowing
from dopant gas containers to vapor-phase growth apparatus by reducing
said dopant gas pressure.
2. Description of the Prior Art
A well known prior art gas supplying apparatus is configured such that
chemical processing gas, filled as compressed gas or liquefied gas in a
gas container or gas cylinder, is supplied through piping system via
pressure reducing valve to chemical processing apparatus.
FIG. 4 illustrates the schematic configuration of a vapor-phase growth
plant as an example of such conventional gas supplying apparatus.
According to the drawings, the vapor-phase growth plant has a gas supplying
container(or gas cylinder) 61 which is filled up with dopant gas (for
example, H.sub.2 diluted B.sub.2 H.sub.6 : diborane gas) 62. The dopant
gas flows through a dopant gas supply piping 64 via a pressure reducing
valve 63 to a thin film growth chamber 65a disposed in a vapor-phase
growth apparatus 65. In the thin film growth chamber 65a, the dopant gas
is supplied on a substrate which is loaded in the chamber for growing thin
film by vapor-phase growth on the surface of the substrate.
For the purpose of removing any contaminants in the dopant gas supply
piping 64 which may intrude from surroundings, a gas purging apparatus is
connected to the dopant gas supply piping 64. The gas purging apparatus is
equipped a purging gas supplying conduit 66 and a purging gas discharge
conduit 67 respectively therewith.
As for purging gas, nitrogen gas (N.sub.2) or rare gas (Ar, He etc.) are
adopted. The part which is closed by a dotted line in the FIG. 4 shows
cylinder cabinet 68 for storing the gas supplying container 61.
As shown above, in the prior art, the cylinder cabinet 68 is disposed on
one-for-one correspondence to the vapor-phase growth apparatus 65. The
reason for this is that a gas supplying container commonly used, as usual,
has some variance in dopant gas concentration. Therefore, upon replacing
of the dopant gas supplying container, dopant gas concentration may vary
for some extent, which may result in variance on atomic concentration of
the grown thin film produced in the vapor-phase growth apparatus 65,
though operated in the same situation or the same film growing condition.
In consequence, to avoid undesirable variance of dopant concentration in
the grown thin film caused by replacing the dopant gas supplying
container, thin film growth condition by the vapor-phase growth apparatus
must be adjusted respectively in accordance with the dopant gas
concentration of each dopant gas supplying container.
However, since the cylinder cabinet 68 is disposed on one-for-one
correspondence to the vapor-phase growth apparatus 65 in the conventional
vapor-phase growth plant, the following problem arise:
(1) As the number of vapor-phase growth apparatus 65 increases, the number
of cylinder cabinet 68 must be increased, which results in the increase of
plant installation cost.
(2) In order to avoid variance in grown thin film quality (dopant
concentration) upon replacing of gas supplying containers, the production
condition must be adjusted, which result in the lesser productivity
because of the increase of adjusting time.
(3) Upon replacing of gas supplying containers, such troublesome operations
as the substituting of residual gas in the dopant gas supplying pipe with
the purging gas would be required.
(4) Ever since the gas supplying container is rather small in volume,
duration on continuous operation is short.
SUMMARY OF THE INVENTION
The present invention, produced in the light of the true state of prior art
described above, has for an object thereof for providing a gas supplying
system which enables to supply highly homogenized high pressure gas in
terms of its concentration together with its pressure, stably and for a
long period to chemical processing apparatus.
Another object of the invention is to improve productivity of chemical
processing apparatus.
Still another object of the invention is to realize simplified operation of
gas supplying apparatus.
A further substantial object of the invention is to provide vapor-phase
growth plant for capable of stable production of qualified thin film with
lesser variance in its quality.
The first aspect of the invention resides in a gas supplying apparatus for
supplying high pressure gas flowing from gas supplying containers which
are filled said gas therein, through gas conduction means being equipped
pressure reducing valves therewith, to at least one chemical processing
apparatus, which gas supplying apparatus is characterized by comprising a
plurality of gas supplying containers each of which having outlet for
simultaneous supplying of the gas flow therefrom, and a gas conduction
means for conducting the gas flow having a plurality of gas supply
conduits being connected to each outlet of the gas supplying containers
therewith, which gas supply conduits forming a multiple stage network with
a plurality of confluence to merge and to unite the gas supply conduits
respective thereat along with the gas flow direction, thereby reducing the
number of gas supply conduits, which the final stage of the multiple stage
network being formed at the final stage confluence single gas supply
conduit thereof, being connected through at least one pressure reducing
valve at least one of chemical processing apparatus therewith, whereby
enabling gas flow rate of each gas container being flown out therefrom to
even, by making even of pressure drop within the gas supply conduits
jointly connected between each of the outlet of each gas container and the
final stage conflux therethrough.
The second aspect of the invention resides in a gas supplying apparatus set
forth in the first aspect of this invention, wherein the gas conduction
means of which the gas supply conduits comprising a multiple stage
tournament-style network, by merging and uniting the gas supply conduits
on the respective confluence.
The third aspect of the invention resides in a gas supplying apparatus set
forth in the first or second aspect of this invention, further comprising
at least one gas buffering means being disposed by insertion between an
outlet of the pressure reducing valve at the final stage confluence and
the respective chemical processing apparatus therewith.
The fourth aspect of the invention resides in a gas supplying apparatus set
forth in the first or second or third aspect of this invention, further
comprising at least one gas purging apparatus being equipped with at least
one purging gas supplying conduit and with at least one purging gas
discharge conduit and with at least one decompression exhaust conduit.
The fifth aspect and function of the invention resides in a gas supplying
apparatus set forth in any of the first to fourth aspect of this
invention, in which each gas supplying conduit having the same inner
diameter and the same length and the same bending configuration so as to
even pressure drop within the gas conduction means disposed between each
gas supplying container and respective confluence.
The sixth aspect and function of the invention resides in a gas supplying
apparatus set forth in any of the first to fifth aspect of this invention,
in which high pressure gas being dopant gas, and the chemical processing
apparatus being vapor-phase growth apparatus.
The seventh aspect of the invention resides in a vapor-phase growth plant
having at least one gas supplying container being filled up with high
pressure dopant gas therein to flow therefrom, at least one vapor-phase
growth apparatus and a dopant gas conduction means together with at least
one pressure reducing valve thereof, for growing of thin film in the
presence of the dopant gas supplied therefrom through the dopant gas
conduction means on respective substrate disposed within respective
vapor-phase growth apparatus, which vapor-phase growth plant is
characterized by comprising a plurality of dopant gas supplying containers
each of which having outlet for simultaneous supplying of the dopant gas
flow therefrom, and a gas conduction means for conducting the dopant gas
flow having a plurality of gas supply conduits being connected to each
outlet of the dopant gas supplying containers therewith, which gas supply
conduits forming a multiple stage network with a plurality of confluence
to merge and to unite the gas supply conduits respective thereat along
with the gas flow direction, thereby reducing the number of gas supply
conduits, which the final stage of the multiple stage network being formed
at the final stage confluence single gas supply conduit thereof, being
connected through at least one pressure reducing valve at least one of
vapor-phase growth apparatus therewith, whereby enabling dopant gas flow
rate of each gas supplying container being flown out therefrom to even, by
making even of pressure drop within the gas supply conduits jointly
connected between each of said outlet of each gas supplying container and
the final stage confluence therethrough.
Moreover, as the substantial example of high pressure gas, dichlorosilane
or monosilane are applicable as gas phase raw material to be used for
vapor-phase growth of thin film, while phosphine, diboran, arsine or
others are also applicable as dopant gas which are added for vapor-phase
growth of thin film.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be better understood and the objects and features
thereof other than those set forth above will become apparent when
consideration is given to the following detailed description thereof,
which makes reference to the following drawings, wherein:
FIG. 1 is a flowsheet illustrating an example of the vapor-phase growth
plant according to the present invention.
FIG. 2 is a plan view illustrating the essential part of an example of
substantial gas conduction means according to the present invention to
even dopant gas pressure drop between each gas supplying containers and
each confluences, with three gas supplying containers equipped.
FIG. 3 is a plan view illustrating the essential part of an another example
of substantial gas conduction means according to the present invention to
even dopant gas pressure drop between each gas supplying containers and
each confluence, with eight gas supplying containers equipped.
FIG. 4 is a flow sheet for representing of a prior art vapor-phase growth
plant.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
This invention will more specifically be described below with reference to
the preferred embodiments illustrated in the drawings annexed hereto, a
vapor-phase growth plant having at least one thin film vapor-phase growth
apparatus which correspond to the chemical processing apparatus described
above, for growing thin film layer on a substrate therein, in the presence
of high pressure dopant gas which also corresponds to the high pressure
supplying gas described above.
FIG. 1 is a flow sheet of a vapor-phase growth plant for production of thin
film having a dopant gas supplying system and thin film vapor-phase growth
apparatus.
As shown in the FIG. 1, the vapor-phase growth plant comprises eight gas
supplying containers denoted by notation 200a, 200b, 200c, 200d, 200e,
200f, 200g, 200h respectively which contain high pressure dopant gas 1,
four vapor-phase growth apparatus denoted by notation 41a, 41b, 41c and
41d for growing of thin film, plural of dopant gas supply conduits denoted
by notation 30a, 30b, 30c, 30d, 30e, 30f, 30g, 30h, 30j, 30k, 30m, 30n,
3a, 3b, 4c, 3d, 3e, 3f and 3g which jointly connect between each of the
gas containers (200a to 200h), with each of growth vessels (not shown)
equipped in each of the vapor-phase growth apparatus (41a to 41d).
The gas supply conduits construct a multiple stage gas flow subsystem which
corresponds to the gas conduction means described above, a four-stage gas
flow subsystem in this case, which successively connects and merges the
gas supply conduits from upper gas flow to down gas flow along with the
gas flow direction, thereby reducing gradually the number of gas supply
conduits so as to shape a tournament-diagram-style network of which paths
gradually decrease from the upper end to the down end.
The gas supply conduits 30a, 30b, 30c, 30d, 30g, 30h, 30j and 30k form the
first stage of the multiple stage gas flow subsystem, disposed at the
upper end of the subsystem, which of each end connecting to the outlet of
each gas containers (200a to 200h).
Every two of the first stage gas supply conduits in pair are connected and
united to one of second stage conduit (30e, 30f, 30m or 30n), thereby
reducing the number of the second stage conduit to half.
For example, two of the first stage gas supply conduits 30a and 30b in pair
are connected and united on a first stage confluence 4a, to a second stage
gas conduit 30e thereat.
Similarly two of the first stage gas supply conduits 30c and 30d in pair
are connected and united on a first stage confluence 4b, to a second stage
gas conduit 30f thereat.
Also, a pair of the first stage gas supply conduits 30g and 30h connecting
and uniting on a first stage confluence 4c to a second stage gas conduit
30m, and a pair of the first stage gas supply conduits 30j and 30k
connecting and uniting on a first stage confluence 4d to a second stage
gas conduit 30n thereat.
Successively, every two of the second stage gas supply conduits in pair are
connected and united to one of third stage conduit, thereby reducing the
number of the third stage conduit to half.
For example, two of the second stage gas supply conduits 30e and 30f in
pair are connected and united on a second stage confluence 5a, to a third
stage gas conduit 3a thereat. The gas conduit 3a is then connected via a
pressure reducing valve 9 to a third stage gas conduit 3b.
In the same manner two of the second stage gas supply conduits 30m and 30n
in pair are connected and united on a second stage confluence 5b, to a
third stage gas conduit 3c thereat. The gas conduit 3c is then connected
via a pressure reducing valve 10 to a third stage gas conduit 3d.
Finally, the two of the third stage gas supply conduits in pair are
connected and united to a fourth (or final) stage conduit, thereby
reducing the number of the final stage conduit to half: more specifically
the two of the second stage gas supply conduits 3b and 3d are connected
and united on a third stage confluence 6, to a final stage gas conduit 3e
thereat.
Though the configuration shown above provides eight gas containers, there
exist no restrictions in the number of gas supplying containers, together
with the number of gas flow stages: for example, twenty or more gas
containers are applicable.
Several of thin film growth chambers are commonly equipped, but not
restricted in total number of these.
On the downstream side of the third stage gas supply conduit 3a, a primary
pressure reducing valve 9 is disposed while the outlet of the primary
pressure reducing valve 9 is connected with a gas supply conduit 3b, of
which the opposite end connecting to a two way valve 7 which enabling
fully opened or fully closed of gas flow pass.
The output from the two way valve 7 is conducted to the third stage
confluence 6.
Likewise to the above, on the downstream side of the third stage gas supply
conduit 3c, a primary pressure reducing valve 10 is disposed while the
outlet of the primary pressure reducing valve 10 is connected with a gas
conduit 3d, of which the opposite end connecting to a two way valve 8
which enabling fully opened or fully closed of gas flow pass. The output
from the two way valve 8 is conducted also to the third stage conflux 6.
With the configuration described above, the primary pressure reducing valve
9 (or 10) is placed on the upper stream side while the two way valve 7 (or
8) is placed on the down stream side, in tandem connection: contrary to
this, a reverse configuration of arranging the two way valve 7 (or 8) on
the upper stream side while the primary pressure reducing valve 9 (or 10)
on the down stream side in tandem connection is also applicable.
In parallel to the primary pressure reducing valve 9 or 10, another two way
valve (not shown) enabling fully opened or fully closed of gas flow pass
can also be disposed.
With the two way valve and the primary pressure reducing valve 9 or 10, the
dopant gas can be supplied through either the primary pressure reducing
valve 9 or 10, or bypassing through the two way valve, to the succeeding
stage.
On the down stream side of the final stage where two of the gas supply
conduit 3b and 3d are merged to a sole gas supply conduit 3e, a secondary
reducing valve 11 is disposed connecting its inlet to the down end of the
gas supply conduit 3e. Also, the outlet of the secondary reducing valve 11
is connected with a gas conduit 3f of which the opposite end connecting to
a buffer tank 12. A gas supply conduit 3g connects between the outlet of
the buffer tank 12 and each inlet of four units of vapor-phase growth
apparatus 41a, 41 b, 41c and 41d.
The gas supply conduits (3a to 3d and 30a to 30n) which connect between
each gas supplying containers (200a to 200h) and the two way valves (7 and
8) are connected with a gas purging apparatus comprising of a purging gas
supply conduit 22 and with a purging gas discharge conduit 23 and with a
decompression exhaust conduit 24.
Notations 22a, 22b, 22c and 22d denote two way valves which are connected
to the purging gas supply conduit 22 while notations 23a, 23b, 23c and 23d
denote two way valves which are connected to the purging gas discharge
conduit 23, and notations 24a, 24b, 24c and 24d denote two way valves
which are connected to the decompression exhaust conduit 24, and notations
25, 26 and 27 denote pressure gauges respectively. Notation 51 denotes an
ejector, a turbo molecular pump for example.
It is desirable for the gas supply conduits (3a to 3g and 30a to 30n), or
for the gas supply conduits (22 to 24), or for the valves equipped to
those conduits and also for the buffer tank 12 to be formed of which inner
surface with electrolytic polished SUS316.
By use of the electrolytic polished SUS316, it is advantageous not only
preventing corrosion of their inner surface but also preventing
contaminants charged from the inner surface of these to intrude into the
gas flow of each conduits. Thus, the vapor growth plant is constructed
with a dopant gas supplying apparatus 31 of which components include the
gas supplying containers (200a to 200h), the multiple stage gas flow
subsystem having the gas supply conduits (3a to 3g and 30a to 30n), the
valves (9 to 11), the gas buffering means 12 and the ejector 51, and with
the vapor-phase growth apparatus (41a to 41d).
Next, the working and its resultant effect of this embodiment are described
below.
The operation for dopant gas supply noted below uses at once all of the
eight gas supplying containers (200a to 200h) to supply dopant gas.
Preceding to explain the preferred operating condition, an undesirable
operating condition is firstly described: if the primary pressure reducing
valves 9 and 10 are used under simultaneous use of all the eight gas
supplying containers, a small pressure difference between these two valves
may occur, and by the pressure difference, though small in extent, causes
gas flow rate difference from the pressure reducing valve with higher
pressure to increase than that from the pressure reducing valve with lower
pressure, which in consequence may fail to even each dopant gas flow rate
supplied from these eight gas supplying containers.
Therefore, with the preferred operating condition of this invention, the
above described two way valves which are equipped in parallel to the
primary pressure reducing valves 9 and 10 are used, instead of using the
primary pressure reducing valves 9 and 10.
On the production of thin film under the vapor deposition process by
applying diborane gas (B.sub.2 H.sub.6) as its dopant 1, the two way
valves 7 and 8 are fully opened while all of cocks of the eight gas
supplying containers (200a to 200h) filled with diborane gas (B.sub.2
H.sub.6) of 120 kg/cm.sup.2 are also opened.
The dopant gas 1 flown out from the left four gas supplying containers
200a, 200b, 200c and 200d into the gas supply conduit 3a are merged and
mixed during flowing the conduit therein: more specifically, each dopant
gas flow from the two of gas supplying containers 200a and 200b via the
gas supply conduits 30a and 30b are merged and mixed on the confluence 4a
to unite one stream in the gas supply conduits 30e while each dopant gas
flow from the two of gas supplying containers 200c and 200d via the gas
supply conduits 30c and 30d are merged and mixed on the confluence 4b to
unite one stream in the gas supply conduits 30f, and then the generated
two streams in the gas supply conduits 30e and 30f are merged and mixed on
the confluence 5a to unite one stream which flows into the gas supply
conduit 3a.
The gas stream in the gas supply conduit 3a then passes through the two way
valve equipped in parallel to the pressure reducing valve 9 and flows into
the gas supply conduit 3b. The gas stream in the gas supply conduit 3b
then passes through the two way valve 7 and is conducted to the confluence
6.
On the other hand, the dopant gas 1 flown out from the right four gas
supplying containers 200e, 200f, 200g and 200h into the gas supply conduit
3c are also merged and mixed during flowing the conduit therein: more
specifically, each dopant gas flow from the two of gas supplying
containers 200e and 200f via the gas supply conduits 30g and 30h are
merged and mixed on the confluence 4c to unite one stream in the gas
supply conduits 30m while each dopant gas flow from the two of gas
supplying containers 200g and 200h via the gas supply conduits 30j and 30k
are merged and mixed on the conflux 4d to unite one stream in the gas
supply conduits 30n, and then the two streams generated are merged and
mixed on the confluence 5b to unite one stream which flows also into the
gas supply conduit 3c. The gas stream in the gas supply conduit 3c then
passes through the two way valve equipped in parallel to the pressure
reducing valve 10 and flows into the gas supply conduit 3d. The gas stream
in the gas supply conduit 3d then passes through the two way valve 8 and
is conducted to the confluence 6.
Further, both of the gas stream are then merged and mixed on the conflux 6
to unite one stream which flows into the gas supply conduit 3e. The mixed
gas flow through passing of the gas supply conduit 3e is then subjected to
the secondary pressure reducing valve 11 to reduce its pressure to 4
kg/cm.sup.2, and flows into the gas supply conduit 3f. The decompressed
gas stream in the gas supply conduit 3f is dividedly supplied to each
vapor-phase growth apparatus (41a to 41d) via the gas buffer tank 12.
In the embodiment described above, each of dopant gas flow rate from each
of eight gas supplying containers (200a to 200h) can be kept even, with
merging and mixing them under a tournament-style networking manner above
described.
This can also more effectively be attained with every gas supplying conduit
to the respective confluence having the same inner diameter and the same
length and the same bending configuration, so as to even each pressure
drop to the respective confluence.
In consequence, each of the dopant gas flow from each of gas supplying
container can offset gas concentration variance each other via gas supply
conduits and respective confluences, which results in dopant gas supplying
with lesser concentration variance.
Moreover, with more compact piping, saving space of piping can be attained.
Thus, with the multiple stage gas flow subsystem described above, an
equalized constant flow rate of dopant gas from each of gas supplying
containers can be supplied to respective confluence, and at once in the
confluence each of the dopant gas flow can offset gas concentration
variance each other to even, dopant gas with lesser concentration variance
can be supplied. As a result, the system is able to supply a determined
concentration of dopant gas flow in stable and for longer period, to the
vapor-phase growth apparatus (41a to 41d).
Effective embodiments of substantial configuration of gas conduction means
to even pressure drop from the gas supplying containers to the respective
confluence are illustrated by their plan view in FIG. 2 and FIG. 3.
The embodiment shown in the FIG. 2 has three gas supplying containers 2, 2
and 2 connected by three gas supply conduits 2a, 2a and 2a which are
united to a confluence 2b. The three gas supply conduits 2a, 2a and 2a
have the same inner diameter, the same length and the same bending
configuration.
The embodiment shown in the FIG. 3 has eight gas supplying containers 2, 2,
2, 2, 2, 2, 2 and 2 connected by eight gas supply conduits 2a, 2a, 2a, 2a,
2a, 2a, 2a and 2a which are united to a confluence 2b, of which the eight
gas supply conduits 2a, 2a, 2a, 2a, 2a, 2a, 2a and 2a have the same inner
diameter, the same length and the same bending configuration.
Also by disposing a primary pressure reducing valve and a secondary
pressure reducing valve in series, dopant gas pressure for supplying to
vapor-phase growth apparatus can more stably be controlled to a
predetermined value.
Since the system shown in the FIG. 1 has two groups of conduits (or piping)
which are disposed in parallel, continuous operation can be attained by
the following switching schedule of dopant gas supply: With this case,
primary pressure reducing valves 9 and 10 are used. This operation
schedule enjoys better operability than the previous operation schedule
described heretofore with simultaneous use of all of eight gas supplying
containers.
According to this operation schedule, during a former half operation
period, the two way valve 7 is opened while the two way valve 8 is closed,
thereby using solely the left four gas supplying containers 200a, 200b,
200c and 200d simultaneously. And when their residual pressure decrease to
around 10 kg/cm.sup.2, the former half operation period is terminated:
then the operation proceeds to a latter half operation period, where the
two way valve 7 is closed while the two way valve 8 is opened, thereby
using solely the right four gas supplying containers 200e, 200f, 200g and
200h simultaneously.
While proceeding the latter half operation period, the four exhausted gas
supplying containers 200a, 200b, 200c and 200d are replaced to new ones
with dopant gas pressure of 120 kg/cm.sup.2. Thus, by changing
alternatively the four gas supplying containers to another four new ones,
the two groups of gas supplying containers can effectively be used in
turn.
In order to execute automatically the switching operation between the two
groups of gas supplying containers, it is desirable to equip Pressure
Indication Controllers (PIC) disposed to the primary circuit of the
primary pressure reducing valves 9, 10 and replacing the said two way
valves 7,8 to solenoid control valves respectively, by connecting each
operation part of the said solenoid control valve to the said PIC.
With the configuration, immediate after detecting by the PIC the pressure
to decrease to 10 kg/cm.sup.2 for example, the two solenoid control valves
are switched over, to control one of them being opened while the other
being closed.
By request, an appending two way valve can be disposed on the gas supply
conduit 3e in addition to the two way valves 7 and 8. Or a new two way
valve can be disposed on the gas supply conduit 3e by removing the
existing two way valves 7 and 8. In the latter case, however, dopant gas
flow cannot be switched.
During replacement of a gas supplying container at the gas supply conduits
3a or 3c, contaminants, dust or other undesirable particles clinging to
worker's wear may intrude via opening to those conduits. In such cases
according to the invention, the above described gas purging apparatus
having a purging gas supplying conduit 22 and a purging gas discharge
conduit 23 and a decompression exhaust conduit 24 is used.
For example upon replacing the left four exhausted gas supplying containers
200a, 200b, 200c and 200d, firstly the two way valve 7 is closed, and just
before or just after releasing of the gas supply conduits (30a to 30d) to
remove from these containers, among twelve in total two way valves (22a to
24d), the two way valves 22a, 22b, 23a and 23b to be full opened while the
rest of them to be full closed. With this operation, nitrogen gas is
supplied as a purging gas through the purging gas supplying conduit 22
into the gas supply conduits (3a, 3b, and 30a to 30d) while a part of
nitrogen gas in these gas supply conduits is discharged from both of each
open end of the four gas supply conduits (30a to 30d) and the open end of
the purging gas discharge conduit 23.
During this operation the left four exhausted gas supplying containers
200a, 200b, 200c and 200d are replaced to the new four gas supplying
containers which are filled up dopant gas at a pressure of 120
kg/cm.sup.2, and after their replacement all of the cock of these gas
supplying containers to be full closed. By this operation, the nitrogen
gas cleans the inner side of the gas supply conduits (3a, 3b, and 30a to
30d), also preventing contaminants to intrude into the gas supplying
containers 200a, 200b, 200c and 200d through the container-side end of the
gas supply conduits (30a to 30d).
After closing the two way valves 22a, 22b, 23a and 23b, starts the ejector
51 thereby discharging residual nitrogen gas in the gas supply conduits
(3a, 3b, and 30a to 30d) through the decompression exhaust conduit 24. On
this discharging, among twelve in total two way valves (22a to 24d) the
two way valves 24a and 24b to be full opened while the rest of them to be
full closed.
The discharging operation continues till the pressure in the conduit
reaches to 10.sup.-4 to 10.sup.-5 Torr, for example. Then the all cock of
the newly installed gas supplying containers to be full opened, thereby
holding high pressure state in the gas supply conduits (30a to 30d, 30e,
30f and 3a).
According to the vapor-phase growth plant illustrated in the FIG. 1, which
has a dopant gas supplying apparatus comprising a plurality of dopant gas
supplying containers, and a multiple stage gas flow subsystem with a
plurality of dopant gas supply conduits therein, of which said dopant gas
supply conduits form a tournament-like network with a plurality of
confluences on which the dopant gas supply conduits are united and the gas
flows therein are merged for subjection to even mixing, which results in
gradual decreasing of the number of the dopant gas supply conduits as the
dopant gas flows proceed in the multiple stage gas flow subsystem.
Since the buffer tank is equipped together with the pressure reducing
valves, the dopant gas which is highly evened its pressure and its
concentration can be supplied to the vapor-phase growth apparatus, thereby
affording stable production of vapor-phase growth products with extremely
lessened quality variance.
The dopant gas supplying apparatus described compiles the gas supply
conduits within it to divide into two groups, each of which can be used
alternatively by switching of these. Therefore, the system can supply
dopant gas continuously and for a longer period. Also the operation of the
dopant gas supplying apparatus can be simplified.
The dopant gas supplying apparatus described above also has a buffer tank
and two stage pressure reducing valves in tandem connection. Upon
alternative use of the above described two groups by switching operation,
the two stage pressure reducing valves suppress dopant gas pressure
fluctuation which may occur due to the switching. Also, the buffer tank
works to prevent the impact of pressure fluctuation which may occur due to
ON/OFF operation of some vapor-phase growth apparatus, to influence to
other vapor-phase growth apparatus.
Thus, the dopant gas supplying apparatus of this invention can supply high
pressure dopant gas with highly evened for both in its concentration and
its pressure, stably and successively for a longer period to the chemical
processing apparatus.
Also, since the dopant gas supplying apparatus of this invention is
equipped with a gas purging apparatus having purging gas supplying means,
purging gas discharge means and decompression exhaust means, the system is
free from intruding by contaminants in the gas supply conduits upon
replacement of the gas supplying containers. With this function, there is
no need to perform test production after replacing of the gas supplying
containers for examining the quality and for adjusting production
condition to maintain its quality, thereby greatly improve productivity.
Also, the dopant gas supplying apparatus can perform the gas purging
operation and the decompression exhaust operation to many gas supplying
containers at once, the efficiency of gas supplying container replacement
operation improves significantly.
This invention will be described more specifically below with reference to
the working examples illustrated in the drawings annexed hereto.
EXAMPLE
As shown in the FIG. 1, eight gas supplying containers of 47 liter capacity
for each filled with hydrogen diluted diborane gas (B.sub.2 H.sub.6) were
set to a vapor-phase growth plant. The concentration and pressure of the
diborane gas in the right four gas supplying containers were, (96.0 ppm,
122 atm ), (98.5 ppm, 121 atm), (101.0 ppm, 121 atm), (103.5 ppm, 122 atm)
while those in the left four gas supplying containers were (96.5 ppm, 121
atm ), (99.0 ppm, 121 atm), (100.5 ppm, 122 atm), (104.5 ppm, 121 atm),
respectively.
During one month operation as the former half period, the right four gas
supplying containers were used. By setting the primary pressure of the
pressure reducing valve 10 to 8 kg/cm.sup.2, the secondary pressure of the
pressure reducing valve 11 to 4 kg/cm.sup.2 respectively, the B.sub.2
H.sub.6 gas were supplied to four vapor-phase growth apparatus 41a, 41b,
41c and 41d, each of which is one-piece type equipped with two units of
growing vessels in it.
At the two vapor-phase growth apparatus 41a and 41b, SiHCl.sub.3
(Trichlorosilane) gas and B.sub.2 H.sub.6 gas were supplied to single
crystalline p-type silicon substrate with resistivity ranges from 0.01 to
0.02 ohm.multidot.cm, thickness of 725 micrometer, and 200 mm in diameter,
under growth temperature of 1100 centigrade with growth rate of 4.0
micrometer/min, for obtaining of single crystalline p-type silicon thin
film with the target thickness of 6 micrometer and the target resistivity
of 6 ohm.multidot.cm.
Also, at the rest two vapor-phase growth apparatus 41c and 41d, the same
gas described above were supplied to single crystalline p-type silicon
substrate with the same specification described above under the same
growth condition described above, for obtaining of single crystalline
p-type silicon thin film with the target thickness of 4 micrometer and the
target resistivity of 2 ohm.multidot.cm.
In this case, for attaining of the target resistivity, dopant gas flow rate
supplied to the vapor-phase growth apparatus 41a, 41b, 41c and 41d were 62
cc/min, 60 cc/min, 191 cc/min and 187 cc/min respectively, which values
were set according to their characteristic tables.
After the one month operation (the former half of period ) of single
crystalline p-type silicon thin film growth, the right four B.sub.2
H.sub.6 gas supplying containers were switched to the left four gas
supplying containers, and the latter half period of successive one month
was started. In the latter case, the primary gas pressure of the pressure
reducing valve 9 were set to 8 kg/cm.sup.2 for supplying B.sub.2 H.sub.6
gas to all the vapor-phase growth apparatus 41a, 41b, 41c and 41d, while
the film growth condition were set to same to the former half of period.
After the two-months operation, the resistivity of the grown thin films
were examined by Hg probe method. The sampling wafers were extracted at
intervals of 25 wafers produced in each of the vapor-phase growth
apparatus. The sampling points atom for each sampling wafer were the
center of the wafer, and the four points at the inner positions radially
10 mm apart from the outer edge, the five resulted points in total for
each wafer.
By measuring these, the average resistivity of the five sampling points for
each substrate are listed in TABLE 1. In the table, each variance of
resistivity (%) is obtained by the following equation;
((Average resistivity in the latter half period-Average resistivity in the
former half period )/Average resistivity in the former half
period).times.100
TABLE 1
______________________________________
Vapor-phase
Average resistivity
Average resistivity
Variance
Growth in the former
in the latter
of
Apparatus
half period half period resistivity
______________________________________
41a 6.02 ohm .multidot. cm
6.02 ohm .multidot. cm
+1.0%
41b 6.01 ohm .multidot. cm
6.06 ohm .multidot. cm
+0.8%
41c 1.98 ohm .multidot. cm
2.01 ohm .multidot. cm
+1.5
41d 2.01 ohm .multidot. cm
2.03 ohm .multidot. cm
+1.0%
______________________________________
As shown in the TABLE 1, the variance of resistivity attains as small value
as .+-.1.5%, at its maximum. Thus, by applying the plant illustrated in
the FIG. 1, it is ascertained that the single crystalline silicon thin
film of lesser resistivity variance can be produced without altering the
growth condition (dopant gas flow rate, for example), though the gas
supplying containers were switched during the two-month of film growth
duration.
Comparative Example
A gas supplying container of 47 liter capacity filled with hydrogen diluted
diborane gas (B.sub.2 H.sub.6) was set to a vapor-phase growth plant shown
in the FIG. 4. The concentration and pressure of the diborane gas in the
gas supplying container were 103.0 ppm and 122 atm.
By setting the secondary pressure of the pressure reducing valve 63 to 4
kg/cm.sup.2, the B.sub.2 H.sub.6 gas was supplied to the vapor-phase
growth apparatus 65 of one-piece type equipped with two units of growing
vessels in it.
At the vapor-phase growth apparatus 65, SiHCl.sub.3 (Trichlorosilane) gas
and B.sub.2 H.sub.6 gas were supplied to single crystalline p-type silicon
substrate with its resistivity ranging from 0.01 to 0.02 ohm.multidot.cm,
thickness of 725 micrometer, and 200 mm in diameter, under growth
temperature of 1100 centigrade with growth rate of 4.0 micrometer/min, for
obtaining of single crystalline p-type silicon thin film with the target
thickness of 4 micrometer and the target resistivity of 2 ohm.multidot.cm.
In this case, for the purpose of setting of the growth condition, the
relations between dopant gas flow rate and thin film resistivity had
previously been investigated by test running.
With three times of the test running, the adequate dopant gas flow rate for
attaining the target resistivity was found to be 181 cc/min. The obtained
gas flow rate was consequently adopted to this reaction.
After the one month operation, the resistivity of the grown thin films were
examined by Hg probe method. The sampling wafers were extracted at
intervals of 25 wafers produced in the vapor-phase growth apparatus 65.
The sampling point for each sampling substrate were the same to that in
the Example 1 described above.
By measuring these, the average resistivity of the five sampling points was
1.99 ohm.multidot.cm.
On continuing a month of thin film growth, the pressure of the B.sub.2
H.sub.6 supplying container was degraded below 10 atm, therefore it was
replaced to another container of which B2H6 concentration and pressure
were 97.0 ppm and 121 atm. By setting the secondary pressure of the
pressure reducing valve 63 to 4 kg/cm.sup.2, and by setting also the
growth condition to the same to those described above, 25 wafers in total
were produced.
By extracting one wafer among these 25 wafers, resistivity of the grown
film were measured with the same method described above. The measured
average resistivity of the five sampling points was 2.12 ohm.multidot.cm,
which suffering of large increase of .+-.6.5%.
Therefore the production was ceased at that point, and twice of test
running were attempted. By the test run, the adequate doping gas flow rate
for the new gas supplying container was confirmed to 192 cc/min. Under
this growth condition, additional 1000 wafers were produced. By extracting
one sample wafer for every 25 produced wafers, 40 sampling wafers were
obtained. The measured average resistivity of the five sampling points for
each wafer was 2.01 ohm.multidot.cm, which showed a decrease to the
previous desirable value.
As already obvious by the explanation above, an important advantage of this
invention is for enabling supply of high pressure gas with highly evened
for both in its concentration and its pressure, stably and successively
for a longer period to the chemical processing apparatus.
Another advantage of this invention is for enabling stable production of
vapor-phase growth products with extremely lessened their variance in
quality.
A further advantage of this invention is for realizing the improved
simplified operation of the gas supplying apparatus, and there is no need
to perform test production after replacing of the gas supplying containers
for examining the quality.
Another advantage of this invention is for enabling continuous chemical
processing for a longer period, thereby greatly improve productivity.
A further advantage of this invention is for enabling the efficiency of gas
supplying container replacement operation to improve significantly.
Having illustrated and described the principles of the invention in a
preferred embodiment thereof, it should be readily apparent to those
skilled in the art that the invention can be modified in arrangement and
detail without departing from such principles. We claim all of
modifications coming within the spirit and scope of the accompanying
claims.
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